Production of brown shades on the fiber.



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'HENBE SCHMIID, OF III'U'LHAUSEN, GERMANY, ASSIG-NOR TO BADISCHE ANILIN &- SODA FABRIK, 0F. LUDWIGSHAFEN-ON-THE-RHINE, GERMANY, A CORPORATION.

PRUIDUCTION 0F BRO'WN SHADES ON THE FIBER.

amines.

1W0 Drawing.

To all whom may concern:

, of which the following is a specification.

In the specification of Letters Patent No. 863,? 61 isdescribed the production of brown shades by oxidizing, on fibrous material by means of a chlorate in the presence of a vanadium salt, para-phenylene-diamin, or a homologue, or isomer, thereof, without sufiicient mineral acid to combine with the whole thereof. This process, however, has the disadvantage that the shade of brown obtained cannotbe sufiiciently varied. I have now discovered that various shades of brown can be obtained if, when carrying out the aforesaid process, instead of para-phenylene'diamin alone, a mixture thereof with an aminohydroxy compound be employed. When carrying out the process of this invention, both the para-phenylene-diamin body and the amino-hydroxy compound should be employed so that the whole thereof, or at any rate the greater part thereof, is in the form of the free base. When using such mixture of a para-phenylene-diamin body and an amino-hydroxy compound, results are obtained which cannot be obtained by the use of either of these constituents separately. For instance, although meta-aminophenol when oxidized by itself on the material yields a light brown-violet shade, if it be oxidized in the presence of a limited quantity of para phenylene diamin, the shade produced is dark olive-brown. If a mixture of para-phenylene-diamin, orthoamino-phenol, and meta-amino-phenol be employed, the brown compound produced has a yellowish tinge, whereas a'mi'xture of para phenylene diamin and ort-ho aminophenol gives rise td a garnet shade of brown. Similarly, by taking other mixtures of para phenylene-diamin, or ahomologue, or isoe mer, thereof, with an amino-hydroxy-compound, other shades of brown can be obtained which are all fast againstthe action of washing and light. In each case varieated, or discharge, effects can be produced if desired. I U

The following are examples of the preparation of baths in accordance with my in- Specificatien of Letters Patent.

Patented Dec. 5, 1911i.

Application filed November 30, 1909. Serial No. 530,658.

vention, but the said invention is not limited to these examples.

Example 1-Paddng bath for brown.- Dissolve ten grams of para-phenylene-diamin, four grams of ortho-amino-phenol, two grams of meta-amino-phenol, sixteen grams of ammonium chlorid, and sixteen grams of sodium chlorate, in water, add fifteen cubic centimeters of one per thousand ammonium vanadate solution, and make up the whole to one liter. If necessary, filter the solution The bath can be used either before, or after, dilution.

E wample 2-Padding bath for fawn c0Z0r.--Dissolve nine grams of para phenylenediamin, five grams of meta-amino-phenol, one gram of ortho-amino-phenol, twenty grams of ammonium chlorid, and twenty grams of sodium chlorate in water, and add sixteen cubic centimeters of a one per thousand ammonium vanadate solution. Make up the whole to one liter and filter the solution, if necessary.

E'azample 3-Padding bath for olivebrown.-Dissolve seven grams of para-phenylene-diamin, seven grams of meta-amino phenol, twenty grams of ammonium chlorid, and twenty grams of sodium chlorate in water, add sixteen grams of ammonium vanaplate solution, and make up the whole to one iter.

The material, after being padded, or otherwise treated, with either of the aforesaid baths, should be dried rapidly, without being heated too strongly, and can the? be steamed in a Mather-Flatt apparatus, for example, if a uniform shade be des red.

Either white, or colored, discharge eflects can be obtained, for example, in a manner similar to that described in the aforesaid specification of Letters Patent No. $63,761.

It is sometimes useful to add say from thirty to forty cubic centimeters of glycerintartar-emetic solution to each liter of'the printing or padding solution. The glycerin-tartar-emetic solution can be prepared by dissolving forty grams of tartar emetic in six hundred and twenty cubic centimeters of hot water and three hundred and forty grams of glycerin.

Now what I claim is 1. The process of producing brown shades body and an amino-hydroxy body, a chlorate and a vanadium eon'ipound, at least one-half of the amino groups bein in the tree state, and then causing the oxication ot the paraphenylene-diamin body and of the amino hydroxy body substantially. as described.

2. The process of producing brown shades on the fiber by applying to the material a mixture containing para-pheny1ene-diamin and an amino-phenol and a chlorat* and a vanadium compound, at least one-half of the amino groups being in the free state, and then causing the oxidation of the paraphenylene-diamin and of the amino-phenol substantially as described.

3. The process of producing brown shades on the fiber by applying to the material a mixture containing a para-phenylene-diami 11 body and an an'lino-hydroxy body, a ehlo rate and a vanadium compound, at least onehalf of the amino groups being in the free state, then drying the material and subjecting it to the action of steam.

4-, The process of producing brown shades with discharge effects on the fiber by applying to the ma rial a mixture containing a para-phenyle e-diamin body and an aminohydroxy body, a chlorate and a vanadiinn compound, at least one-half of the amino groups being in the free state, then drying the material and printing W1th a paste con- 1,01 ose taining a reducing agent and then subjecting it to the action of steam.

The process of producing brown shades with discharge etl ects on the fiber by applying to the material a mixture containing a para-phony]ene-diamin body and an aminohydroxy body, a glyeeriii-tartar emetic solution, a chlorate and a vanadium compound, at least one-half of the amino groups being in the free state, thendrying the material, printing it with a paste containing a reduo ing agent and then subjecting it to the action of stean'i.

t. The process of producing brown shades with discharge eltccts on the fiber by applying to the material a mixture containing a. para-phenylene-diamin body and an aminolrvdroxy body, a glycerin-tartar emetic solution, a chlorate and a vanadium compound,

at least one hal't of the amino grtmps being in the free state, then drying the material,

printing it with a paste containing a reducing agent and a coloring matter, and then subjecting it to the action of steam.

In testimony whereof I have hereunto set my hand in the presence of two subseribing witnesses.

. HENRI SCHMID. Witnesses Gisonon G'irrono, ARNOLD ZUnnn.

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